Method for preparing thesium Chinese turcz total flavone
A technology of baleen grass and total flavonoids, which is applied in the field of traditional Chinese medicine preparation, can solve the problems of unclear effective parts, low content of total flavonoids, etc., and achieves the effects of high yield and simple process
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example 1
[0018] Take the dried herbal herb, crush it through a 40-mesh sieve, weigh 25g, add 500ml of 70% ethanol, heat and reflux for extraction for 2 hours, filter, add 250ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove residue, and combine The filtrate was left to stand for 12 hours, centrifuged at 4000 rpm for 10 minutes, the supernatant was taken, ethanol was recovered under reduced pressure, and dried under reduced pressure at 40°C. Dissolve the crude extract in 60ml of 95% ethanol, add dropwise 20ml of 1% basic lead acetate aqueous solution while stirring, let it stand for 0.5 hours, and precipitate; % sodium carbonate aqueous solution 10ml, stand still for 0.5 hours, precipitate, filter, add dilute hydrochloric acid to the filtrate to adjust the pH value to neutral, recover ethanol under reduced pressure, add water to 60ml, add 120ml n-butanol to extract twice, recover n-butanol under reduced pressure , dried under reduced pressure at 40° C. to obtain 2.12 g...
example 2
[0020] Take the dried herbal herb, crush it through a 40-mesh sieve, weigh 5g, add 100ml of 70% ethanol, heat to reflux for 2 hours, filter, add 50ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove residue, and combine the filtrate , stand still for 12 hours, centrifuge at 4000 rpm for 10 minutes, take the supernatant, recover ethanol under reduced pressure, add water to the remaining liquid to 50ml, put 100g of processed HZ-80 macroporous adsorption resin chromatography column, after adsorption , add distilled water to wash until the effluent is colorless, then wash the column with 60% ethanol at 10ml / min until the effluent has no flavonoid reaction. The above 60% ethanol effluents were combined, the ethanol was recovered under reduced pressure, and dried under reduced pressure at 40° C. to obtain 0.235 g of brown-red powder with a yield of 4.7% (based on crude drug). Aluminum trichloride develops color, and the content determined by spectrophotometry is 19.7...
example 3
[0022] Take the dried herbal herb, crush it through a 40-mesh sieve, weigh 10g, add 200ml of 70% ethanol, heat to reflux for 2 hours, filter, add 100ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove residue, and combine the filtrate , stand still for 12 hours, centrifuge at 4000 rpm for 10 minutes, take the supernatant, recover ethanol under reduced pressure, and obtain 3.5g extract after drying under reduced pressure at 40°C; Stir the amide powder evenly, and dry at 50°C; after drying, put the powder on a polyamide resin chromatography column with 4 times the amount, add distilled water to wash until the effluent is colorless, and then use 30% ethanol, 50% ethanol and 70% ethanol in sequence, 10ml / min washes the chromatographic column, simultaneously with thymelin I, thymelin II and thymelin III as reference substance, and thin-layer chromatography detects the effluent composition; Merging contains a large amount of thymelin flavonoid fractions, reducing Th...
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